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Parameter
Method Performance
Please
report in units as stated in SMPR!
Weighting
factor for
parameter
Suitability Ranking (1‐
3‐5)
(select from drop‐down
list, 5 = best)
SPIFAN matrices
Applicable to all forms of infant, adult, and/or pediatric formula
(powders, ready‐to‐feed liquids, and liquid concentrates).
Any combination of milk, soy, rice, whey, hydrolyzed protein,
starch, and amino acids, with and without intact protein.
The method is applicable to all the matrices listed
in the SMPR.
1
All analytes defined in the
applicability statement are
measured.
1
Analyte 1
trans‐vitamin K1 = 1‐100 mcg/100g recostituted sample
trans‐vitamin K1 = 0.5‐100 mcg/100g
Analyte 2
cis‐vitamin K1 = 1‐100 mcg/100g recostituted sample
cis‐vitamin K1 = 0.1‐100 mcg/100g
Analyte 3
Total‐vitamin K1 = 1‐100 mcg/100g recostituted sample
Total‐vitamin K1 = 0.6‐100 mcg/100g
Analyte 4
Analyte 5
Analyte 1
trans‐vitamin K1 = <1 mcg/100g recostituted sample
trans‐vitamin K1 = 0.5 mcg/100g
Analyte 2
cis‐vitamin K1 = <1mcg/100g recostituted sample
cis‐vitamin K1 = 0.1/100g
Analyte 3
Total‐vitamin K1 = <1mcg/100g recostituted sample
Total‐vitamin K1 = 0.6mcg/100g
Analyte 4
Analyte 5
Spike recovery (%) Vitamin K1 (cis + trans) = 90‐100%
Vitamin K1 (cis + trans) = 97.8 + 5.2% (n=44)
2
Bias vs SRM NIST SRM 1849a Vitamin K1 = 1.06 + 0.17 mg/Kg
NIST SRM 1849a Vitamin K1 = 1.00 + 0.10 mg/Kg
(n=5)
3
<8% RSD
<5% RSD
1‐10 mcg/100g
<8% RSD
7.90%
>10 mcg/100g
<5% RSD
6.30%
b
Units
Analytical Range.
1
Method title:
Principle of the method:
A LC‐MS/MS Method for Vitamin K Analysis in Infant Formula and Adult Nutrition Samples
Fat in sample is hydrolyzed by lipase after adding internal std. Vitamin K is extracted by a solvent extraction. The reconstituted extract is analyzed by LC‐MS/MS for vitamin K.
SMPR Requirement
Evaluation of Method Performance vs. SMPR requirements.
Feedback from Users of the Method since being awarded
First Action
Official Methods
Status
Repeatability (RSDr)
Reproducibility (RSDR)
Accuracy/Recovery
Blank check and lowest and midrange calibration
ADDITIONAL EVALUATION PARAMETERS
Intermediate Reproducibility
(RSDiR)
Limit of quantification (LOQ)
Method Reference #
VITK‐01
AOAC SMPR: ………….. AOAC SMPR 2014.001
Limit of detection (LOD)
1
a
Concentrations apply to (1) "ready to feed liquids" "as‐is"; (2) reconstituted powders (25 g into 200 g water); and (3) liquid concentrates diluted 1:1 by weight.
Did Method Author Consider ERP’s Method Specific
Recommendations
(See web link to specific method
comments):
Decision by ERP
Proprietary equipment
Notes:
Overall Score
Recommendation of ERP
2 years after First Action Status
Laboratory safety
Other Considerations
3
1
2
move to Final Action/repeal/remove/expand 2 year term
0
No unique proprietary equipment/accessories are required.
Method does not require any special safety precautions e.g. personal protection from highly toxic solvents.
Bias against established method
Analytical equipment
1
Adequate proof of performance via system suitability
Is there a bias Yes/No ?
Analytical equipment is commonly available in most labs.
SPIFAN ERP Checklist v 1.6
27.06.2013
VitK-01 MEF
FOR ERP USE ONLY
DO NOT DISTRIBUTE